In this work, in order to prevent agglomeration of SiO 2 in the poly(amide-imide) (PAI) matrix, the surface of SiO 2 was modified with bio-active citric acid (CA) to obtain SiO 2 /CA. Then, the PAI was synthesized from the polymerization reaction of biosafe and optically active diacid with 4,4?-diamino diphenylether using molten tetra-n-butylammonium bromide as green solvent and triphenyl phosphite. Then, the SiO 2 /CA were incorporated into the obtained optically active PAI and PAI-SiO 2 /CA nanocomposites (PSCN)s were prepared via a fast ultrasonic irradiation process. Finally, the SiO 2 /CA and PSCNs were characterized by different methods such as FT-IR, XRD, FE-SEM, TEM and TGA techniques. According to FE-SEM and TEM micrographs the distribution of SiO 2 in the polymer matrix was homogeneous. In the second project, the SiO 2 were modified with poly(vinyl alcohol) (PVA). Then, the modified SiO 2 with PVA (SiO 2 -PVA) were incorporated into the PAI matrix for the preparation of PAI-SiO 2 -PVA NCs (PSiPN)s. Finally, the resulting SiO 2 -PVA and PSi were characterized by different analyses. TGA data showed high thermal stability of the obtained PSi compared to the pure PAI. TEM images of SiO 2 -PVA demonstrated most of the SiO 2 -PVA particles are spherical in shape with very good dispersion.